CN109679528A - A kind of toilet seat hot-fusible pressure-sensitive adhesive and preparation method thereof - Google Patents
A kind of toilet seat hot-fusible pressure-sensitive adhesive and preparation method thereof Download PDFInfo
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- CN109679528A CN109679528A CN201910033804.4A CN201910033804A CN109679528A CN 109679528 A CN109679528 A CN 109679528A CN 201910033804 A CN201910033804 A CN 201910033804A CN 109679528 A CN109679528 A CN 109679528A
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- parts
- sensitive adhesive
- toilet seat
- fusible pressure
- styrene
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J109/00—Adhesives based on homopolymers or copolymers of conjugated diene hydrocarbons
- C09J109/06—Copolymers with styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to macromolecule adhesive technical fields, and in particular to arrives a kind of toilet seat hot-fusible pressure-sensitive adhesive and preparation method thereof.The toilet seat hot-fusible pressure-sensitive adhesive, including hydrogenation C5/C9 copolymerized petroleum resin.Toilet seat hot-fusible pressure-sensitive adhesive prepared by the present invention can have excellent cohesive strength while keeping excellent coating performance, meanwhile, product of the present invention has preferable wellability to substrate, and usage experience sense is excellent in.
Description
Technical field
The invention belongs to macromolecule adhesive technical fields, more particularly it relates to which a kind of toilet seat heats
Pressure sensitive adhesive and preparation method thereof.
Background technique
Disposable closestool pad hot-fusible pressure-sensitive adhesive is to be used to be coated on disposable closestool pad material surface, primary applied to preventing
Gliding dislocations of the property closestool cushion material in plastics toilet seat, hot melt adhesive for fixing.
However, market starts to occur better using skin-friendly now with the raising that people require usage comfort
Non-woven fabrics material replaces paper-like materials to make disposable closestool pad.But due to the stiction force of skin-friendly material and skin very great Cheng
Degree is greater than the stiction force of material and toilet seat, largely affects the usage experience of user.In consideration of it, being produced to improve
The usage experience of product needs a kind of harmless and environmentally friendly hot-fusible pressure-sensitive adhesive, improves closestool cushion material and closestool
Washer stiction force, while when opening without hot melt glue residua.
Summary of the invention
To solve the above-mentioned problems, the first aspect of the invention provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, system
Standby raw material includes hydrogenation C5/C9 copolymerized petroleum resin.
As a kind of perferred technical scheme, the raw material for preparing of the toilet seat hot-fusible pressure-sensitive adhesive further includes modified virtue
Fragrant race C9 Petropols.
As a kind of perferred technical scheme, the hydrogenation C5/C9 copolymerized petroleum resin and modified aromatic race C9 petroleum tree
The weight ratio of rouge is 1:(1.5-2.5).
As a kind of perferred technical scheme, the raw material for preparing of the toilet seat hot-fusible pressure-sensitive adhesive further includes benzene second
Alkene-acrylates.
As a kind of perferred technical scheme, the styrene-propene hydrochlorate is styrene-propene acid sodium-salt.
As a kind of perferred technical scheme, the raw material for preparing of the toilet seat hot-fusible pressure-sensitive adhesive further includes SBR rubber
Glue, naphthenic oil, antioxidant.
As a kind of perferred technical scheme, by weight, the toilet seat hot-fusible pressure-sensitive adhesive prepares raw material
Including following component: hydrogenation 8-15 parts of C5/C9 copolymerized petroleum resin, 20-25 parts of modified aromatic race C9 Petropols, styrene-
3-5 parts of acrylates, 22-30 parts of SBR rubber, 10-20 parts of naphthenic oil, 0.5-1 parts of antioxidant.
As a kind of perferred technical scheme, by weight, the toilet seat hot-fusible pressure-sensitive adhesive prepares raw material
Including following component: hydrogenation 10-14 parts of C5/C9 copolymerized petroleum resin, 21-24 parts of modified aromatic race C9 Petropols, styrene-
3.5-4.5 parts of acrylates, 24-28 parts of SBR rubber, 12-18 parts of naphthenic oil, 0.5-0.8 parts of antioxidant.
As a kind of perferred technical scheme, by weight, the toilet seat hot-fusible pressure-sensitive adhesive prepares raw material
Including following component: hydrogenation 12 parts of C5/C9 copolymerized petroleum resin, 23 parts of modified aromatic race C9 Petropols, Styrene And Chloroalkyl Acrylates
4 parts of salt, 26 parts of SBR rubber, 15 parts of naphthenic oil, 0.7 part of antioxidant.
The second aspect of the invention provides a kind of preparation method of toilet seat hot-fusible pressure-sensitive adhesive, and step includes:
It (1) will be in the naphthenic oil, antioxidant investment stainless steel cauldron；
(2) after being warming up to 140 DEG C, SBR rubber is added, and temperature of reaction kettle is controlled at 150 DEG C；
(3) after SBR rubber is completely dissolved investment hydrogenation C5/C9 copolymerized petroleum resin, modified aromatic race C9 Petropols,
The temperature of stainless steel cauldron is controlled and stirs 30-60min within 200 DEG C by styrene-propene hydrochlorate, be evacuated to-
0.085MPa, discharge cooling packing.
The utility model has the advantages that toilet seat hot-fusible pressure-sensitive adhesive prepared by the present invention can keep excellent coating performance
Meanwhile there is excellent cohesive strength, meanwhile, product of the present invention has preferable wellability, usage experience sense performance to substrate
It is excellent.
Specific embodiment
It is further clear, complete that the technical characteristic work in technical solution is provided to the present invention With reference to embodiment
Description, not to the limitation of its protection scope.
Word " preferred ", " preferred " in the present invention etc. refer to, can provide in some cases certain beneficial to effect
The embodiment of the present invention of fruit.However, other embodiments are also likely to be preferred under identical circumstances or in the case of other
's.In addition, do not imply that other embodiments are unavailable to the statement of one or more preferred embodiments, be also not intended to by
Other embodiments exclude except the scope of the present invention.
When a numberical range disclosed herein, above range is considered as continuously, and the minimum value including the range and most
Big value and each value between this minimum value and maximum value.Further, when range refers to integer, including the model
Each integer between minimum value and maximum value enclosed.In addition, when providing multiple range Expressive Features or characteristic, Ke Yihe
And the range.In other words, unless otherwise specified, otherwise all ranges disclosed herein are understood to include and are wherein included into
Any and all subrange.For example, should be regarded as including between minimum value 1 and maximum value 10 from the specified range of " 1 to 10 "
Any and all subrange.The Exemplary range of range 1 to 10 include but is not limited to 1 to 6.1,3.5 to 7.8,5.5 to
10 etc..
To solve the above-mentioned problems, the first aspect of the invention provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, system
Standby raw material includes hydrogenation C5/C9 copolymerized petroleum resin.
Hydrogenate C5/C9 copolymerized petroleum resin
Petropols (hydrocarbon resin) of the present invention are C5, C9 fraction of petroleum cracking institute by-product, before menstruation
A kind of thermoplastic resin of the techniques production such as processing, polymerization, distillation, its not instead of high polymer, molecular weight is between 300-3000
Oligomer.Petropols are divided into group aliphatic resin (C5), alicyclic resin (DCPD), aromatic resin according to the difference of raw material
(C9), aliphatic/aromatic copolymer resins (C5/C9) and hydrogenated petroleum resin.
Hydrogenation C5/C9 copolymerized petroleum resin of the present invention and the compatibility of high polymer matrix are good, and price is low, therefore quilt
For a variety of industries such as rubber, adhesive, coating, papermaking, ink and field.
In a preferred embodiment, hydrogenation C5/C9 copolymerized petroleum resin of the present invention is available commercially from South Korea
Can be grand, the trade mark is the product of SU-400；SU-400 is considered as the product that softening point is 97-107 DEG C of softening point.
In a preferred embodiment, the raw material for preparing of toilet seat hot-fusible pressure-sensitive adhesive of the present invention further includes
Modified aromatic race C9 Petropols.
Modified aromatic race C9 Petropols
C9 Petropols of the present invention are being catalyzed using the by-product C9 fraction of cracking ethylene preparation device as primary raw material
It polymerize in the presence of agent, or it is subjected to thermoplastic resin prepared by combined polymerization with aldehydes, aromatic hydrocarbons, terpene compound.C9 stone
Polar functionalities are not having with good water resistance, resistance to acid and alkali, weatherability and light fastness aging in the structure of oleoresin
Dissolubility in solvent is good, good with the compatibility of other resins, also enbrittles, tackifying, caking property and plasticity.
Modified aromatic race C9 Petropols of the present invention, and aliphatic hydrocarbon and aromatic hydrocarbon favorable solubility, compatibility compared with
It is good.
In a preferred embodiment, modified aromatic race C9 Petropols of the present invention be available commercially from the U.S. she
The graceful chemistry of scholar, the trade mark are the product of PiccoAR85；PiccoAR85 is considered as the product that softening point is 87 DEG C.
In a preferred embodiment, hydrogenation C5/C9 copolymerized petroleum resin of the present invention and modified aromatic race C9
The weight ratio of Petropols is 1:(1.5-2.5).
Present inventor has found that the present invention has preferable tack in the course of the study, is due to phase between the two
Capacitive is preferable, and softening point is close, not only improves processing viscosity, and make the dispersibility of modified aromatic race C9 Petropols compared with
Good, so that intermolecular force greatly reinforces, cohesive force is higher.And when hydrogenation C5/C9 copolymerized petroleum resin and modified aromatic race
The weight ratio 1:(1.5-2.5 of C9 Petropols), the present invention has preferable caking property.
In a preferred embodiment, the raw material for preparing of toilet seat hot-fusible pressure-sensitive adhesive of the present invention further includes
Styrene-propene hydrochlorate.
Styrene-propene hydrochlorate
Styrene-propene hydrochlorate of the present invention refers to that styrene monomer, which is completed acid monomers progress free radical with unsaturation, to be total to
Poly-, reaction generates copolymer, then in the solution or molten by the oxide of copolymer and metal, hydroxide or acetate etc.
It is reacted under state, obtains ionomer.
In a preferred embodiment, styrene-propene hydrochlorate of the present invention is styrene-propene acid sodium-salt.
In a preferred embodiment, the preparation step of styrene-propene acid sodium-salt of the present invention includes:
(1): a certain amount of initiator azo-bis-isobutyl cyanide (AIBN), monomer styrene and propylene being added in four-hole boiling flask
Acid makees solvent with benzene, after letting nitrogen in and deoxidizing 30min, carries out heating water bath, and temperature is 75 DEG C, reacts 6h, total overall reaction process is in nitrogen
It is carried out under gas shielded；
(2): after reaction, reactant being poured into petroleum ether precipitation 24 hours, copolymer is then obtained by filtration, in vacuum
70 DEG C of baking oven carry out thousand dry, then are purified gained copolymer 3 times with dioxane/water, to remove unreacted acrylic acid and instead
The acrylate homopolymer that should be generated is dried to obtain one acrylic copolymer of styrene after purification；
(3): weighing above-mentioned copolymer and be dissolved in dioxane, use NaOH/CH3OH solution is neutralized, dry, so that it may to obtain
Styrene-propene acid sodium-salt.
Wherein, the molar ratio of the acrylic acid and styrene is 1:(2-5)；The AIBN accounts for the 3wt% of monomer.
Present inventor has found in the course of the study, not only may be used using styrene-propene hydrochlorate described herein
To increase the dispersibility of system, and make that there is preferable compatibility between each component, to make the processing performance of product more
Add brilliance.Surprisingly, when using styrene-propene hydrochlorate of the present invention, the bonding of product can be enhanced
Performance, and make product that there is preferable wellability to substrate.Inventor speculates, the possible reason is styrene-propene hydrochlorate
It interacts with resin system, forms multiple ion to aggregation, to generate micro phase separation structure, improve cohesive force.And by
In the presence of phenyl ring, so that peripheral motor is limited layer and overlaps, play certain supporting role so that surface distribution largely with
Interaction the preferable resin material of wellability.
In a preferred embodiment, the raw material for preparing of toilet seat hot-fusible pressure-sensitive adhesive of the present invention further includes
SBR rubber, antioxidant, naphthenic oil.
SBR rubber
Butadiene-styrene rubber (SBR) of the present invention, also known as polystyrenebutadienes copolymer.Its physical mechanism performance, processing
Performance and the service performance of product are close to natural rubber, some performances are for example wear-resisting, heat-resisting, ageing-resistant and curingprocess rate is more natural
Rubber is more excellent, can be used in combination with natural rubber and various synthetic rubber, be widely used in tire, adhesive tape, sebific duct, wire and cable,
The fields such as the production of medical apparatus and various rubber products are the largest general purpose synthetic rubber kind, and realize industry earliest
One of the rubber clone that metaplasia produces.
In a preferred embodiment, SBR rubber of the present invention is purchased from the limited public affairs of Yueyang Ba Ling Huaxing petrochemical industry
Department, trade mark SBS-1401.
Naphthenic oil
It has the cyclic carbon chain structure and saturation branch of saturation to naphthenic oil of the present invention, because this structure, makes
Naphthenic oil had not only had some properties of arene, but also some properties with straight-chain hydrocarbons, therefore had preferably between rubber
Compatibility.In addition, there is low pour point, high density, high viscosity, the spies such as have no toxic side effect again since naphthenic oil comes from natural oil
Point, it is cheap, from the horse's mouth the advantages that, production cost can be effectively reduced.
In a preferred embodiment, naphthenic oil of the present invention is limited available commercially from the Nanjing vast petrochemical industry of letter
Company, the trade mark are the product of K10B.
Antioxidant
Antioxidant of the present invention is a kind of auxiliary agent generally used in adhesive, and the use of antioxidant not only can be with
The thermal oxide of material in process is reduced, chemical stability is improved, material can also be slowed down in use due to light
According to flavescence, aging etc. caused by temperature change.
In some embodiments, antioxidant of the present invention is selected from phenolic antioxidant, amine antioxidants, sulphur class antioxygen
One of agent, phosphite ester antioxidant are a variety of.
In a preferred embodiment, antioxidant of the present invention be antioxidant 1010 and irgasfos 168 by weight
Than compounding to obtain for 1:1.
In a preferred embodiment, by weight, the toilet seat hot-fusible pressure-sensitive adhesive prepares raw material
Including following component: hydrogenation 8-15 parts of C5/C9 copolymerized petroleum resin, 20-25 parts of modified aromatic race C9 Petropols, styrene-
3-5 parts of acrylates, 22-30 parts of SBR rubber, 10-20 parts of naphthenic oil, 0.5-1 parts of antioxidant.
In a preferred embodiment, by weight, the toilet seat hot-fusible pressure-sensitive adhesive prepares raw material
Including following component: hydrogenation 10-14 parts of C5/C9 copolymerized petroleum resin, 21-24 parts of modified aromatic race C9 Petropols, styrene-
3.5-4.5 parts of acrylates, 24-28 parts of SBR rubber, 12-18 parts of naphthenic oil, 0.5-0.8 parts of antioxidant.
In a preferred embodiment, by weight, the toilet seat hot-fusible pressure-sensitive adhesive prepares raw material
Including following component: hydrogenation 12 parts of C5/C9 copolymerized petroleum resin, 23 parts of modified aromatic race C9 Petropols, Styrene And Chloroalkyl Acrylates
4 parts of salt, 26 parts of SBR rubber, 15 parts of naphthenic oil, 0.7 part of antioxidant.
The second aspect of the invention provides a kind of preparation method of toilet seat hot-fusible pressure-sensitive adhesive, and step includes:
It (1) will be in the naphthenic oil, antioxidant investment stainless steel cauldron；
(2) after being warming up to 140 DEG C, SBR rubber is added, and temperature of reaction kettle is controlled at 150 DEG C；
(3) after SBR rubber is completely dissolved investment hydrogenation C5/C9 copolymerized petroleum resin, modified aromatic race C9 Petropols,
The temperature of stainless steel cauldron is controlled and stirs 30-60min within 200 DEG C by styrene-propene hydrochlorate, be evacuated to-
0.085MPa, discharge cooling packing.
The present invention is specifically described below by embodiment, in addition, if without other explanations, it is raw materials used to be all
It is commercially available.
Embodiment
Embodiment 1
Embodiment 1 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
8 parts of resin, 3 parts of styrene-propene hydrochlorate, 22 parts of SBR rubber, 10 parts of naphthenic oil, resists 20 parts of modified aromatic race C9 Petropols
0.5 part of oxidant.
The hydrogenation C5/C9 copolymerized petroleum resin is can be grand available commercially from South Korea, and the trade mark is the product of SU-400.
The modified aromatic race C9 Petropols are available commercially from U.S.'s eastman chemical, and the trade mark is the production of PiccoAR85
Product.
The styrene-propene hydrochlorate is styrene-propene acid sodium-salt, and preparation step includes:
(1): a certain amount of initiator azo-bis-isobutyl cyanide (AIBN), monomer styrene and propylene being added in four-hole boiling flask
Acid makees solvent with benzene, after letting nitrogen in and deoxidizing 30min, carries out heating water bath, and temperature is 75 DEG C, reacts 6h, total overall reaction process is in nitrogen
It is carried out under gas shielded；
(2): after reaction, reactant being poured into petroleum ether precipitation 24 hours, copolymer is then obtained by filtration, in vacuum
70 DEG C of baking oven carry out thousand dry, then are purified gained copolymer 3 times with dioxane/water, to remove unreacted acrylic acid and instead
The acrylate homopolymer that should be generated is dried to obtain one acrylic copolymer of styrene after purification；
(3): weighing above-mentioned copolymer and be dissolved in dioxane, use NaOH/CH3OH solution is neutralized, dry, so that it may to obtain
Styrene-propene acid sodium-salt.
Wherein, the molar ratio of the acrylic acid and styrene is 1:2；The AIBN accounts for the 3wt% of monomer.
The SBR rubber is available commercially from Yueyang petrochemical industry Co., Ltd, Ba Ling Huaxing, and the trade mark is the product of SBS-1401.
The naphthenic oil is available commercially from Nanjing Hong Han petrochemical industry Co., Ltd, and the trade mark is the product of K10B.
The antioxidant is that antioxidant 1010 and irgasfos 168 are that 1:1 compounds to obtain by weight.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive, step include:
It (1) will be in the naphthenic oil, antioxidant investment stainless steel cauldron；
(2) after being warming up to 140 DEG C, SBR rubber is added, and temperature of reaction kettle is controlled at 150 DEG C；
(3) after SBR rubber is completely dissolved investment hydrogenation C5/C9 copolymerized petroleum resin, modified aromatic race C9 Petropols,
The temperature of stainless steel cauldron is controlled and stirs 30min within 200 DEG C by styrene-propene hydrochlorate, be evacuated to-
0.085MPa, discharge cooling packing.
Embodiment 2
Embodiment 2 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
15 parts of resin, 25 parts of modified aromatic race C9 Petropols, 5 parts of styrene-propene hydrochlorate, 30 parts of SBR rubber, 20 parts of naphthenic oil,
1 part of antioxidant.
The hydrogenation C5/C9 copolymerized petroleum resin is can be grand available commercially from South Korea, and the trade mark is the product of SU-400.
The modified aromatic race C9 Petropols are available commercially from U.S.'s eastman chemical, and the trade mark is the production of PiccoAR85
Product.
The styrene-propene hydrochlorate is styrene-propene acid sodium-salt, and preparation step includes:
(1): a certain amount of initiator azo-bis-isobutyl cyanide (AIBN), monomer styrene and propylene being added in four-hole boiling flask
Acid makees solvent with benzene, after letting nitrogen in and deoxidizing 30min, carries out heating water bath, and temperature is 75 DEG C, reacts 6h, total overall reaction process is in nitrogen
It is carried out under gas shielded；
(2): after reaction, reactant being poured into petroleum ether precipitation 24 hours, copolymer is then obtained by filtration, in vacuum
70 DEG C of baking oven carry out thousand dry, then are purified gained copolymer 3 times with dioxane/water, to remove unreacted acrylic acid and instead
The acrylate homopolymer that should be generated is dried to obtain one acrylic copolymer of styrene after purification；
(3): weighing above-mentioned copolymer and be dissolved in dioxane, use NaOH/CH3OH solution is neutralized, dry, so that it may to obtain
Styrene-propene acid sodium-salt.
Wherein, the molar ratio of the acrylic acid and styrene is 1:5；The AIBN accounts for the 3wt% of monomer.
The SBR rubber is available commercially from Yueyang petrochemical industry Co., Ltd, Ba Ling Huaxing, and the trade mark is the product of SBS-1401.
The naphthenic oil is available commercially from Nanjing Hong Han petrochemical industry Co., Ltd, and the trade mark is the product of K10B.
The antioxidant is that antioxidant 1010 and irgasfos 168 are that 1:1 compounds to obtain by weight.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive, step include:
It (1) will be in the naphthenic oil, antioxidant investment stainless steel cauldron；
(2) after being warming up to 140 DEG C, SBR rubber is added, and temperature of reaction kettle is controlled at 150 DEG C；
(3) after SBR rubber is completely dissolved investment hydrogenation C5/C9 copolymerized petroleum resin, modified aromatic race C9 Petropols,
The temperature of stainless steel cauldron is controlled and stirs 60min within 200 DEG C by styrene-propene hydrochlorate, be evacuated to-
0.085MPa, discharge cooling packing.
Embodiment 3
Embodiment 3 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
10 parts of resin, 21 parts of modified aromatic race C9 Petropols, 3.5 parts of styrene-propene hydrochlorate, 24 parts of SBR rubber, naphthenic oil 12
Part, 0.5 part of antioxidant.
The hydrogenation C5/C9 copolymerized petroleum resin is can be grand available commercially from South Korea, and the trade mark is the product of SU-400.
The modified aromatic race C9 Petropols are available commercially from U.S.'s eastman chemical, and the trade mark is the production of PiccoAR85
Product.
The styrene-propene hydrochlorate is styrene-propene acid sodium-salt, and preparation step includes:
(1): a certain amount of initiator azo-bis-isobutyl cyanide (AIBN), monomer styrene and propylene being added in four-hole boiling flask
Acid makees solvent with benzene, after letting nitrogen in and deoxidizing 30min, carries out heating water bath, and temperature is 75 DEG C, reacts 6h, total overall reaction process is in nitrogen
It is carried out under gas shielded；
(2): after reaction, reactant being poured into petroleum ether precipitation 24 hours, copolymer is then obtained by filtration, in vacuum
70 DEG C of baking oven carry out thousand dry, then are purified gained copolymer 3 times with dioxane/water, to remove unreacted acrylic acid and instead
The acrylate homopolymer that should be generated is dried to obtain one acrylic copolymer of styrene after purification；
(3): weighing above-mentioned copolymer and be dissolved in dioxane, use NaOH/CH3OH solution is neutralized, dry, so that it may to obtain
Styrene-propene acid sodium-salt.
Wherein, the molar ratio of the acrylic acid and styrene is 1:3；The AIBN accounts for the 3wt% of monomer.
The SBR rubber is available commercially from Yueyang petrochemical industry Co., Ltd, Ba Ling Huaxing, and the trade mark is the product of SBS-1401.
The naphthenic oil is available commercially from Nanjing Hong Han petrochemical industry Co., Ltd, and the trade mark is the product of K10B.
The antioxidant is that antioxidant 1010 and irgasfos 168 are that 1:1 compounds to obtain by weight.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive, step include:
It (1) will be in the naphthenic oil, antioxidant investment stainless steel cauldron；
(2) after being warming up to 140 DEG C, SBR rubber is added, and temperature of reaction kettle is controlled at 150 DEG C；
(3) after SBR rubber is completely dissolved investment hydrogenation C5/C9 copolymerized petroleum resin, modified aromatic race C9 Petropols,
The temperature of stainless steel cauldron is controlled and stirs 40min within 200 DEG C by styrene-propene hydrochlorate, be evacuated to-
0.085MPa, discharge cooling packing.
Embodiment 4
Embodiment 4 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
14 parts of resin, 24 parts of modified aromatic race C9 Petropols, 4.5 parts of styrene-propene hydrochlorate, 28 parts of SBR rubber, naphthenic oil 18
Part, 0.8 part of antioxidant.
The hydrogenation C5/C9 copolymerized petroleum resin is can be grand available commercially from South Korea, and the trade mark is the product of SU-400.
The modified aromatic race C9 Petropols are available commercially from U.S.'s eastman chemical, and the trade mark is the production of PiccoAR85
Product.
The styrene-propene hydrochlorate is styrene-propene acid sodium-salt, and preparation step includes:
(1): a certain amount of initiator azo-bis-isobutyl cyanide (AIBN), monomer styrene and propylene being added in four-hole boiling flask
Acid makees solvent with benzene, after letting nitrogen in and deoxidizing 30min, carries out heating water bath, and temperature is 75 DEG C, reacts 6h, total overall reaction process is in nitrogen
It is carried out under gas shielded；
(2): after reaction, reactant being poured into petroleum ether precipitation 24 hours, copolymer is then obtained by filtration, in vacuum
70 DEG C of baking oven carry out thousand dry, then are purified gained copolymer 3 times with dioxane/water, to remove unreacted acrylic acid and instead
The acrylate homopolymer that should be generated is dried to obtain one acrylic copolymer of styrene after purification；
(3): weighing above-mentioned copolymer and be dissolved in dioxane, use NaOH/CH3OH solution is neutralized, dry, so that it may to obtain
Styrene-propene acid sodium-salt.
Wherein, the molar ratio of the acrylic acid and styrene is 1:2；The AIBN accounts for the 3wt% of monomer.
The SBR rubber is available commercially from Yueyang petrochemical industry Co., Ltd, Ba Ling Huaxing, and the trade mark is the product of SBS-1401.
The naphthenic oil is available commercially from Nanjing Hong Han petrochemical industry Co., Ltd, and the trade mark is the product of K10B.
The antioxidant is that antioxidant 1010 and irgasfos 168 are that 1:1 compounds to obtain by weight.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive is the same as embodiment 3.
Embodiment 5
Embodiment 5 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
12 parts of resin, 23 parts of modified aromatic race C9 Petropols, 4 parts of styrene-propene hydrochlorate, 26 parts of SBR rubber, 15 parts of naphthenic oil,
0.7 part of antioxidant.
The hydrogenation C5/C9 copolymerized petroleum resin is can be grand available commercially from South Korea, and the trade mark is the product of SU-400.
The modified aromatic race C9 Petropols are available commercially from U.S.'s eastman chemical, and the trade mark is the production of PiccoAR85
Product.
The styrene-propene hydrochlorate is styrene-propene acid sodium-salt, and preparation step includes:
(1): a certain amount of initiator azo-bis-isobutyl cyanide (AIBN), monomer styrene and propylene being added in four-hole boiling flask
Acid makees solvent with benzene, after letting nitrogen in and deoxidizing 30min, carries out heating water bath, and temperature is 75 DEG C, reacts 6h, total overall reaction process is in nitrogen
It is carried out under gas shielded；
(2): after reaction, reactant being poured into petroleum ether precipitation 24 hours, copolymer is then obtained by filtration, in vacuum
70 DEG C of baking oven carry out thousand dry, then are purified gained copolymer 3 times with dioxane/water, to remove unreacted acrylic acid and instead
The acrylate homopolymer that should be generated is dried to obtain one acrylic copolymer of styrene after purification；
(3): weighing above-mentioned copolymer and be dissolved in dioxane, use NaOH/CH3OH solution is neutralized, dry, so that it may to obtain
Styrene-propene acid sodium-salt.
Wherein, the molar ratio of the acrylic acid and styrene is 1:2；The AIBN accounts for the 3wt% of monomer.
The SBR rubber is available commercially from Yueyang petrochemical industry Co., Ltd, Ba Ling Huaxing, and the trade mark is the product of SBS-1401.
The naphthenic oil is available commercially from Nanjing Hong Han petrochemical industry Co., Ltd, and the trade mark is the product of K10B.
The antioxidant is that antioxidant 1010 and irgasfos 168 are that 1:1 compounds to obtain by weight.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive is the same as embodiment 3.
Comparative example 1
Comparative example 1 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
0.1 part of resin, 23 parts of modified aromatic race C9 Petropols, 4 parts of styrene-propene hydrochlorate, 26 parts of SBR rubber, 15 parts of naphthenic oil,
0.7 part of antioxidant.
Raw material is prepared described in comparative example 1 with embodiment 5, the difference is that only parts by weight difference.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive is the same as embodiment 3.
Comparative example 2
Comparative example 2 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
50 parts of resin, 23 parts of modified aromatic race C9 Petropols, 4 parts of styrene-propene hydrochlorate, 26 parts of SBR rubber, 15 parts of naphthenic oil,
0.7 part of antioxidant.
Raw material is prepared described in comparative example 2 with embodiment 5, the difference is that only parts by weight difference.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive is the same as embodiment 3.
Comparative example 3
Comparative example 3 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
12 parts of resin, 0.1 part of modified aromatic race C9 Petropols, 4 parts of styrene-propene hydrochlorate, 26 parts of SBR rubber, 15 parts of naphthenic oil,
0.7 part of antioxidant.
Raw material is prepared described in comparative example 3 with embodiment 5, the difference is that only parts by weight difference.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive is the same as embodiment 3.
Comparative example 4
Comparative example 4 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
12 parts of resin, 50 parts of modified aromatic race C9 Petropols, 4 parts of styrene-propene hydrochlorate, 26 parts of SBR rubber, 15 parts of naphthenic oil,
0.7 part of antioxidant.
Raw material is prepared described in comparative example 4 with embodiment 5, the difference is that only parts by weight difference.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive is the same as embodiment 3.
Comparative example 5
Comparative example 5 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
12 parts of resin, 23 parts of modified aromatic race C9 Petropols, 0.2 part of styrene-propene hydrochlorate, 26 parts of SBR rubber, naphthenic oil 15
Part, 0.7 part of antioxidant.
Raw material is prepared described in comparative example 5 with embodiment 5, the difference is that only parts by weight difference.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive is the same as embodiment 3.
Comparative example 6
Comparative example 6 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
12 parts of resin, 23 parts of modified aromatic race C9 Petropols, 20 parts of styrene-propene hydrochlorate, 26 parts of SBR rubber, 15 parts of naphthenic oil,
0.7 part of antioxidant.
Raw material is prepared described in comparative example 6 with embodiment 5, the difference is that only parts by weight difference.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive is the same as embodiment 3.
Comparative example 7
Comparative example 7 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
12 parts of resin, 23 parts of modified aromatic race C9 Petropols, 4 parts of styrene-propene hydrochlorate, 26 parts of SBR rubber, 15 parts of naphthenic oil,
0.7 part of antioxidant.
Raw material is prepared described in comparative example 7 with embodiment 5, the difference is that, the styrene-propene hydrochlorate is benzene second
Alkene-acrylic acid sodium salt；Monomer described in the preparation step of the styrene-propene acid sodium-salt: mole of acrylic acid and styrene
Than for 0.1:2.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive is the same as embodiment 3.
Comparative example 8
Comparative example 8 provides a kind of toilet seat hot-fusible pressure-sensitive adhesive, including following component: hydrogenation C5/C9 copolymerization petroleum
12 parts of resin, 23 parts of modified aromatic race C9 Petropols, 4 parts of styrene-propene hydrochlorate, 26 parts of SBR rubber, 15 parts of naphthenic oil,
0.7 part of antioxidant.
Raw material is prepared described in comparative example 8 with embodiment 5, the difference is that, the styrene-propene hydrochlorate is benzene second
Alkene-acrylic acid sodium salt；Monomer described in the preparation step of the styrene-propene acid sodium-salt: mole of acrylic acid and styrene
Than for 1:10.
The preparation method of the toilet seat hot-fusible pressure-sensitive adhesive is the same as embodiment 3.
Performance evaluation
1. tensile strength and test of elongation rate: dumbbell shape is made in sample by ASTM-D638-2003, is tested.
2. shear strength test: according to standard ASTM-D1002-72 sample preparation, material PP, overlapping area is 12.5 × 25
(mm2), cooling be placed under test condition is tested after 12h.
3.180 ° of peel strength tests: it is measured by GB/T2792-1998.
Table 1
Claims (10)
1. a kind of toilet seat hot-fusible pressure-sensitive adhesive, which is characterized in that preparing raw material includes hydrogenation C5/C9 copolymerized petroleum resin.
2. toilet seat hot-fusible pressure-sensitive adhesive according to claim 1, which is characterized in that toilet seat hot melt pressure
The raw material for preparing of quick glue further includes modified aromatic race C9 Petropols.
3. toilet seat hot-fusible pressure-sensitive adhesive according to claim 2, which is characterized in that the hydrogenation C5/C9 is copolymerized stone
The weight ratio of oleoresin and modified aromatic race C9 Petropols is 1:(1.5-2.5).
4. toilet seat hot-fusible pressure-sensitive adhesive according to claim 2, which is characterized in that toilet seat hot melt pressure
The raw material for preparing of quick glue further includes styrene-propene hydrochlorate.
5. toilet seat hot-fusible pressure-sensitive adhesive according to claim 4, which is characterized in that the styrene-propene hydrochlorate
For styrene-propene acid sodium-salt.
6. toilet seat hot-fusible pressure-sensitive adhesive according to claim 4, which is characterized in that toilet seat hot melt pressure
The raw material for preparing of quick glue further includes SBR rubber, naphthenic oil, antioxidant.
7. toilet seat hot-fusible pressure-sensitive adhesive according to claim 6, which is characterized in that by weight, the closestool
The raw material for preparing of washer hot-fusible pressure-sensitive adhesive includes following component: hydrogenation 8-15 parts of C5/C9 copolymerized petroleum resin, modified aromatic race
20-25 parts of C9 Petropols, 3-5 parts of styrene-propene hydrochlorate, 22-30 parts of SBR rubber, 10-20 parts of naphthenic oil, antioxidant
0.5-1 parts.
8. toilet seat hot-fusible pressure-sensitive adhesive according to claim 7, which is characterized in that by weight, the closestool
The raw material for preparing of washer hot-fusible pressure-sensitive adhesive includes following component: hydrogenation 10-14 parts of C5/C9 copolymerized petroleum resin, modified aromatic
21-24 parts of race C9 Petropols, 24-28 parts of SBR rubber, 12-18 parts of naphthenic oil, resist 3.5-4.5 parts of styrene-propene hydrochlorate
0.5-0.8 parts of oxidant.
9. toilet seat hot-fusible pressure-sensitive adhesive according to claim 8, which is characterized in that by weight, the closestool
The raw material for preparing of washer hot-fusible pressure-sensitive adhesive includes following component: hydrogenation 12 parts of C5/C9 copolymerized petroleum resin, modified aromatic race C9
23 parts of Petropols, 4 parts of styrene-propene hydrochlorate, 26 parts of SBR rubber, 15 parts of naphthenic oil, 0.7 part of antioxidant.
10. a kind of preparation method of the toilet seat hot-fusible pressure-sensitive adhesive according to any one of claim 6-9, feature
It is, step includes:
It (1) will be in the naphthenic oil, antioxidant investment stainless steel cauldron；
(2) after being warming up to 140 DEG C, SBR rubber is added, and temperature of reaction kettle is controlled at 150 DEG C；
(3) the investment hydrogenation C5/C9 copolymerized petroleum resin, modified aromatic race C9 Petropols, benzene second after SBR rubber is completely dissolved
The temperature of stainless steel cauldron is controlled and stirs 30-60min within 200 DEG C by alkene-acrylates, be evacuated to-
0.085MPa, discharge cooling packing.
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| CN109679528B (en) | 2020-12-01 |
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